Sodium Hydroxide → N-phenyl-1H-imidazol-2-amine
반응식
C(O[CH:4](OCC)[CH2:5][NH:6][C:7]([NH:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=[NH:8])C.[OH-].[Na+]>Cl>[C:10]1([NH:9][C:7]2[NH:8][CH:4]=[CH:5][N:6]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1참가 물질
4
실험 절차
The guanidine (b) was dissolved in HCl (5 mL, 6 M) at 0° C. and then stirred for 2 h. After the starting material was consumed, NaOH (25%) was added until a precipitate formed. This mixture was stirred for 30 min. The reaction was then poured into NaOH (0.5 M), extracted with CH2Cl2, dried and concentrated. Flash chromatography afforded (c) (0.95 g, 50%). NMR (500 MHz, DMSO-d6) δ 8.58 (s, br, 1H), 7.34-6.74 (m, 5H), 6.68 (s, 2H), 6.62 (br, 2H), 3.82 (s, 6H), 3.73 (s, 3H). MS: 157.6 (M−H)−; 160.0 (M+H)+.
후처리
- customAfter the starting material was consumed
- additionNaOH (25%) was added until a precipitate
- customformed
- stirringThis mixture was stirred for 30 min
- extractionextracted with CH2Cl2
- customdried
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-87bf45127d404f68bb690b076455a3b7
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08822513B2
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